Department of Chemical Engineering, Inha University, Incheon, Korea 402-751.
Dalton Trans. 2010 Mar 21;39(11):2883-7. doi: 10.1039/b925088c. Epub 2010 Feb 5.
High quality MOF-177 crystals in the size range of 5-20 microm were successfully synthesized via a sonochemical route in a substantially reduced synthesis time (40 min) in the presence of low-cost NMP (1-methyl-2-pyrrolidone) as a solvent. Microwave heating in NMP also produced MOF-177 under similar conditions (35 min, 5-50 microm) but exhibited inferior crystallinity. In comparison, a conventional solvothermal route in DEF (diethylformamide) took 48 h to produce MOF-177 crystals 0.5-1.5 mm in size. The BET surface areas of the MOF-177 samples decreased in the order of sonochemical (4898 m(2) g(-1)) > conventional (4833 m(2) g(-1)) > microwave route (4197 m(2) g(-1)). In line with this trend, MOF-177 prepared via the sonochemical route resulted in the highest CO(2) adsorption capacity, 1315 mg g(-1) at 30 bar and 298 K. The product yield of MOF-177 synthesized via the sonochemical route was 95.6%, and was significantly higher than the product yields of other methods.
通过超声化学途径，在 NMP（N-甲基-2-吡咯烷酮）作为溶剂的情况下，成功地在大大缩短的合成时间（40 分钟）内合成了尺寸范围在 5-20 微米的高质量 MOF-177 晶体。微波加热在 NMP 下也能在类似条件下（35 分钟，5-50 微米）产生 MOF-177，但结晶度较差。相比之下，在 DEF（二乙基甲酰胺）中的常规溶剂热途径需要 48 小时才能产生 0.5-1.5 毫米大小的 MOF-177 晶体。MOF-177 样品的 BET 表面积按超声化学途径（4898 m(2) g(-1))>常规途径（4833 m(2) g(-1))>微波途径（4197 m(2) g(-1)）的顺序递减。与此趋势一致，通过超声化学途径制备的 MOF-177 具有最高的 CO(2)吸附容量，在 30 巴和 298 K 时为 1315 mg g(-1)。通过超声化学途径合成的 MOF-177 的产物产率为 95.6%，明显高于其他方法的产物产率。
